JP2002180245A - Sputtering target sintered material for photorecording medium protective layer exhibiting excellent cracking damage resistance in high output sputtering condition - Google Patents
Sputtering target sintered material for photorecording medium protective layer exhibiting excellent cracking damage resistance in high output sputtering conditionInfo
- Publication number
- JP2002180245A JP2002180245A JP2000383022A JP2000383022A JP2002180245A JP 2002180245 A JP2002180245 A JP 2002180245A JP 2000383022 A JP2000383022 A JP 2000383022A JP 2000383022 A JP2000383022 A JP 2000383022A JP 2002180245 A JP2002180245 A JP 2002180245A
- Authority
- JP
- Japan
- Prior art keywords
- protective layer
- sputtering
- target material
- medium protective
- high output
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Physical Vapour Deposition (AREA)
- Optical Record Carriers And Manufacture Thereof (AREA)
- Manufacturing Optical Record Carriers (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、半導体レーザー
などの光ビームを用いて、情報の記録や再生、さらに消
去を行う光ディスクなどの光記録媒体の構成層である保
護層をスパッタリング法にて形成するのに用いられるス
パッタリングターゲット焼結材（以下、ターゲット材と
云う）に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for forming a protective layer, which is a constituent layer of an optical recording medium such as an optical disk, on which information is recorded, reproduced, and erased by using a light beam such as a semiconductor laser by a sputtering method. The present invention relates to a sputtering target sintering material (hereinafter, referred to as a target material) used for the sputtering.
【０００２】[0002]
【従来の技術】一般に、上記の光ディスクなどの光記録
媒体が、基本的に例えばポリカーボネイトの基板と、こ
れの表面にいずれもスパッタリング法により形成された
下部保護層、記録層、上部保護層、および反射層の構成
層からなることが知られている。また、上記の光記録媒
体が、例えば図１に概略縦断面図で示される高周波マグ
ネトロンスパッタリング装置を用い、まず、内部を循環
する冷却水によって冷却されたバッキングプレートに所
定の組成をもったターゲット材を取り付け、装置内を真
空排気装置にて排気した後、Ａｒガスを導入して所定の
スッパッタガス圧に保持し、この状態でマッチングボッ
クスを介して設置された高周波電源にてターゲット材に
高周波電力を印加し、これによってターゲット材と、こ
れに対向し、かつ所定の間隔を設けて配置した、例えば
ポリカーボネイトの基板との間にプラズマを発生させ、
このプラズマ中のＡｒイオンをターゲット材の表面に衝
突させてスパッタし、スパッタ粒子を基板表面にそれぞ
れ構成層として蒸着することにより形成されることも知
られている。2. Description of the Related Art Generally, an optical recording medium such as the above-mentioned optical disk is basically composed of, for example, a polycarbonate substrate, and a lower protective layer, a recording layer, an upper protective layer, and a lower protective layer all formed on the surface of the substrate by a sputtering method. It is known that the reflective layer comprises a constituent layer. In addition, the above-mentioned optical recording medium uses, for example, a high-frequency magnetron sputtering apparatus shown in a schematic longitudinal sectional view in FIG. 1, and firstly a target material having a predetermined composition is formed on a backing plate cooled by cooling water circulating inside. After the inside of the apparatus is evacuated by a vacuum evacuation apparatus, Ar gas is introduced and maintained at a predetermined sputter gas pressure, and in this state, high-frequency power is applied to the target material by a high-frequency power supply installed through a matching box. Applied, thereby generating a plasma between the target material and the substrate, for example, polycarbonate, which is opposed to the target material and arranged at a predetermined interval,
It is also known that Ar ions in the plasma collide against the surface of the target material to be sputtered, and sputtered particles are formed on the substrate surface by vapor deposition as constituent layers.
【０００３】さらに、上記の光記録媒体の構成層である
保護層（下部保護層および上部保護層）の形成に、例え
ば特開平６−６５７２５号公報に記載されるように、例
えば原料粉末として、いずれも１０μｍ以下の平均粒径
および９９．９質量％以上の純度を有する酸化けい素
（以下、ＳｉＯ2で示す）粉末および硫化亜鉛（以下、
ＺｎＳで示す）粉末を用い、これら原料粉末を、モル％
で（以下、％はモル％を示す）、ＳｉＯ2：６〜４０
％、ＺｎＳ：残り、の割合に配合し、混合した後、ホッ
トプレス焼結することにより製造されたターゲット材が
用いられていることも知られている。Further, as described in JP-A-6-65725, for example, as a raw material powder, a protective layer (a lower protective layer and an upper protective layer) as a constituent layer of the optical recording medium is formed. Each of them has a silicon oxide (hereinafter referred to as SiO 2 ) powder having an average particle diameter of 10 μm or less and a purity of 99.9 mass% or more, and zinc sulfide (hereinafter, referred to as SiO 2 ).
These raw material powders are represented by mol%
(Hereinafter,% indicates mol%), SiO 2 : 6 to 40
%, ZnS: It is also known that a target material manufactured by blending and mixing in the ratio of remaining, followed by hot press sintering is used.
【０００４】[0004]
【発明が解決しようとする課題】一方、近年の上記の光
ディスクなどの光記録媒体の生産性の向上に対する要求
は強く、これに伴い、構成層の成膜速度も高速化の傾向
にあり、しかし高速成膜を行うためにはターゲット材に
印加する電力を高くして高出力スパッタ条件とする必要
があるが、特に上記の従来ターゲット材を用いて保護層
を形成するに際して、これの高速成膜を行う目的でスパ
ッタ条件を高出力スパッタ条件とすると、ターゲット材
に割れが発生し易くなり、比較的短時間で使用寿命に至
るのが現状である。On the other hand, there is a strong demand for improvement in productivity of optical recording media such as the above-mentioned optical discs in recent years, and accordingly, the film forming speed of the constituent layers tends to be increased. In order to perform high-speed film formation, it is necessary to increase the power applied to the target material to achieve high-output sputtering conditions. In particular, when forming the protective layer using the above-described conventional target material, the high-speed film formation is performed. If the sputtering conditions are set to the high-power sputtering conditions for the purpose of performing the above, cracks are likely to occur in the target material, and the service life is currently reached in a relatively short time.
【０００５】[0005]
【課題を解決するための手段】そこで、本発明者らは,
上述の観点から、上記の光記録媒体保護層形成用の従来
ターゲット材に着目し、これの耐割損性向上を図るべく
研究を行った結果、 （ａ）上記の従来ターゲット材が高速成膜を行う目的で
印加した高スパッタ電力で割れが発生し易いのは、構成
成分であるＺｎＳが同じく構成成分であるＳｉＯ2に比
して高いスパッタ衝撃に対してきわめて脆い性質を有す
ることに原因があること。すなわち高スパッタ電力の印
加でターゲット材表面が受ける高いスパッタ衝撃によっ
てＺｎＳに無数の微細なクラックが発生し、この微細な
クラックが経時的に大きな割れに発展し、この割れで使
用寿命に至ること。Means for Solving the Problems Therefore, the present inventors have proposed:
In view of the above, the present inventors focused on the above-mentioned conventional target material for forming the optical recording medium protective layer, and conducted research to improve the crack resistance thereof. Cracks are likely to occur due to the high sputtering power applied for the purpose of carrying out the process, because ZnS, which is a component, has an extremely brittle property against high sputtering impact as compared with SiO 2 which is also a component. There is. That is, countless fine cracks are generated in ZnS due to high sputter impact applied to the target material surface by application of high sputtering power, and these fine cracks develop into large cracks over time, and the cracks extend the service life.
【０００６】（ｂ）上記の従来ターゲット材に、酸化ラ
ンタン（以下、Ｌａ2Ｏ3で示す）を含有させ、ＺｎＳお
よびＳｉＯ2に加えてＬａ2Ｏ3が共存した組織にする
と、前記Ｌａ2Ｏ3がＺｎＳの受ける高いスパッタ衝撃を
著しく緩和し、これによってＺｎＳにおける微細クラッ
クの発生が抑制され、前記ＳｉＯ2と同じくＬａ2Ｏ3自
身のもつすぐれた耐スパッタ衝撃性と相俟って、この結
果のターゲット材は高出力スパッタ条件下ですぐれた耐
割損性を発揮するようになり、この場合Ｌａ2Ｏ3のター
ゲット材における含有割合が配合割合で６％以下であれ
ば光記録媒体の構成層である保護層（下部保護層および
上部保護層）の特性に何らの悪影響も及ぼさないこと。
以上（ａ）および（ｂ）に示される研究結果を得たので
ある。[0006] (b) in the above conventional target material, lanthanum oxide (hereinafter, La 2 O indicated by 3) is contained, when the tissue in addition to ZnS and SiO 2 is La 2 O 3 coexist, the La 2 O 3 is significantly alleviate the high sputtering shock experienced by the ZnS, whereby the occurrence of fine cracks in the ZnS is suppressed, it sputters resistance impact resistance coupled with the excellent with the same La 2 O 3 itself and the SiO 2, The resulting target material exhibits excellent breakage resistance under high-power sputtering conditions. In this case, if the content ratio of La 2 O 3 in the target material is 6% or less in the mixing ratio, the optical recording medium Have no adverse effect on the characteristics of the protective layers (lower protective layer and upper protective layer) which are the constituent layers of the above.
The research results shown in (a) and (b) above were obtained.
【０００７】この発明は、上記の研究結果に基づいてな
されたものであって、ＳｉＯ2：６〜４０％、Ｌａ
2Ｏ3：１〜６％、ＺｎＳ：残り、からなる配合組成を有
する混合粉末のホットプレス焼結体で構成してなる、高
出力スパッタ条件ですぐれた耐割損性を発揮する光記録
媒体保護層形成用ターゲット材に特徴を有するものであ
る。The present invention has been made on the basis of the above research results, and is based on SiO 2 : 6 to 40%, La
An optical recording medium comprising a hot-press sintered body of a mixed powder having a composition of 2 O 3 : 1 to 6% and ZnS: remaining, and exhibiting excellent crack resistance under high output sputtering conditions. The target material for forming a protective layer has characteristics.
【０００８】なお、光記録媒体保護層形成用ターゲット
材において、ＳｉＯ2の含有割合を配合割合で６〜４０
％にしたのは以下に示す理由からである。すなわち、Ｚ
ｎＳは、光記録媒体保護層に要求される高い光屈折率と
光透過率、さらに耐熱性を具備することから、光記録媒
体保護層の主要成分として用いられているが、反面Ｚｎ
Ｓ単独で例えば光ディスクの保護層を形成した場合、内
部応力の高い保護層となってしまい、この状態で前記光
ディスクに記録のためのレーザー照射を行うと、前記レ
ーザー照射に伴う急熱・急冷によって前記保護層に割れ
が発生し易いものとなる。そこで、光記録媒体保護層で
はＺｎＳにＳｉＯ2を含有させて、保護層中の残留内部
応力を低減するようにしている。したがって、ターゲッ
ト材におけるＳｉＯ2の配合割合が６％未満では、光記
録媒体保護層の含有割合も６％未満となってしまい、前
記保護層における内部応力の発生を抑制する作用が不充
分となり、一方その含有割合が４０％を超えると、同じ
く光記録媒体保護層の含有割合も４０％を超えて高くな
ってしまい、ＺｎＳによってもたらされる上記の特性に
低下傾向が現れるようになることから、その配合割合を
６〜４０％、望ましくは１５〜３０％と定めた。In the target material for forming the protective layer of the optical recording medium, the content ratio of SiO 2 is 6 to 40
The percentage is set for the following reason. That is, Z
nS is used as a main component of the optical recording medium protective layer because it has a high optical refractive index and light transmittance required for the optical recording medium protective layer and further has heat resistance.
For example, when a protective layer of an optical disk is formed by S alone, it becomes a protective layer having a high internal stress, and when laser irradiation for recording is performed on the optical disk in this state, rapid heating and quenching accompanying the laser irradiation cause Cracks are easily generated in the protective layer. Therefore, in the optical recording medium protective layer, ZnS is made to contain SiO 2 to reduce the residual internal stress in the protective layer. Therefore, when the content of SiO 2 in the target material is less than 6%, the content of the optical recording medium protective layer is also less than 6%, and the effect of suppressing the generation of internal stress in the protective layer becomes insufficient. On the other hand, if the content exceeds 40%, the content of the optical recording medium protective layer also becomes higher than 40%, and the above-mentioned characteristics brought by ZnS tend to decrease. The blending ratio was determined to be 6 to 40%, preferably 15 to 30%.
【０００９】さらに、上記ターゲット材のＬａ2Ｏ3の配
合割合を１〜６％にしたのは、その配合割合が１％未満
では、上記の通りＺｎＳに対するスパッタ衝撃緩和作用
を十分に発揮することができず、一方その配合割合が６
％を超えると、光記録媒体保護層の含有割合も６％を超
えて高くなってしまい、ＺｎＳによってもたらされる上
記の特性に低下傾向が現れるようになるという理由から
であり、望ましくは２〜４％とするのがよい。Furthermore, the reason why the mixing ratio of La 2 O 3 in the above-mentioned target material is set to 1 to 6% is that if the mixing ratio is less than 1%, the effect of alleviating the sputtering impact on ZnS is sufficiently exhibited as described above. Cannot be produced, while the mixing ratio is 6
%, The content of the protective layer of the optical recording medium also exceeds 6%, and the above-mentioned properties brought about by ZnS tend to decrease. %.
【００１０】[0010]
【発明の実施の態様】つぎに、この発明の光記録媒体保
護層形成用ターゲット材を実施例により具体的に説明す
る。原料粉末として、３μｍの平均粒径を有する純度：
９９．９９％以上のＺｎＳ粉末、２．５μｍの平均粒径
を有する純度：９９．９％以上のＳｉＯ2粉末、および
０．５μｍの平均粒径を有する純度：９９．９％以上の
Ｌａ2Ｏ3粉末を用意し、これら原料粉末を表１に示され
る配合割合に配合し、これをボールミルにてヘキサン存
在下で４時間混合し、混合後ホットプレート上で８０℃
の温度で乾燥し、さらに４００℃で乾燥し、乾燥後の混
合粉末を黒鉛型に充填した状態でホットプレス装置に装
入し、雰囲気圧力：１．３Ｐａの真空中、温度：１３７
３Ｋ、圧力：３４．３ＭＰａ、保持時間：６時間の条件
で焼結することにより実質的に配合組成と同じ組成を有
し、直径：１２５ｍｍ×厚さ：５ｍｍの寸法をもったホ
ットプレス焼結体からなる本発明ターゲット材１〜９従
来ターゲット材１〜５をそれぞれ製造した。Next, the target material for forming an optical recording medium protective layer according to the present invention will be described in detail with reference to examples. Purity having an average particle size of 3 μm as raw material powder:
99.99% or more ZnS powder, purity with an average particle size of 2.5 μm: SiO 2 powder with 99.9% or more, and purity with an average particle size of 0.5 μm: La 2 with 99.9% or more O 3 powder was prepared, and these raw material powders were mixed in the mixing ratio shown in Table 1, and mixed with a ball mill in the presence of hexane for 4 hours.
, And further dried at 400 ° C., and the mixed powder after drying was charged into a graphite mold and charged into a hot press apparatus, and the atmosphere pressure was 1.3 Pa in a vacuum, and the temperature was 137.
Hot press sintering having substantially the same composition as the compounded composition by sintering under the conditions of 3K, pressure: 34.3 MPa, holding time: 6 hours, and having dimensions of diameter: 125 mm x thickness: 5 mm Inventive target materials 1 to 9 each comprising a body were manufactured.
【００１１】ついで、この結果得られた本発明ターゲッ
ト材１〜９および従来ターゲット材１〜５について、光
記録媒体保護層の特性評価基準となる光屈折率および光
透過率に及ぼす影響を調べた。すなわち、上記の本発明
ターゲット材１〜９および従来ターゲット材１〜５のそ
れぞれを、無酸素銅製の水冷バッキングプレートにハン
ダ付けした状態で、図１に示される構造をもった高周波
マグネトロンスパッタリング装置に装着し、まず装置内
を真空排気装置にて６．７×１０-5Ｐａの真空雰囲気と
した後、Ａｒガスを導入して装置内雰囲気を０．２Ｐａ
のスパッタガス圧とし、引き続いて高周波電源よりマッ
チングボックスを介してターゲット材に１０００Ｗのス
パッタ電力を印加して、前記ターゲット材と対向し、か
つ５０ｍｍの間隔を設けて平行配置した直径：３０ｍｍ
×厚さ：０．５ｍｍのガラス基板と前記ターゲット材間
にプラズマを発生させ、プラズマ中のＡｒイオンを前記
ターゲット材の表面に衝突させて前記ターゲット材をス
パッタし、スパッタ粒子を前記基板表面に蒸着すること
により厚さ：９０ｎｍの光記録媒体保護層を形成した。
この結果形成された光記録媒体保護層の光屈折率および
光透過率を評価する目的で、波長：６３３ｎｍのレーザ
ー光を用い、屈折率および消衰係数を測定した。この測
定結果を表１に示した。Next, the effects of the resulting target materials 1 to 9 of the present invention and the conventional target materials 1 to 5 on the light refractive index and light transmittance, which are the criteria for evaluating the characteristics of the protective layer of the optical recording medium, were examined. . That is, the above-described target materials 1 to 9 of the present invention and the conventional target materials 1 to 5 were soldered to a water-cooled backing plate made of oxygen-free copper, and then applied to a high-frequency magnetron sputtering apparatus having a structure shown in FIG. At first, the inside of the apparatus was set to a vacuum atmosphere of 6.7 × 10 −5 Pa by a vacuum exhaust device, and then the atmosphere in the apparatus was changed to 0.2 Pa by introducing Ar gas.
Then, a sputtering power of 1000 W is applied to the target material from a high-frequency power source through a matching box from a high-frequency power supply, and the diameter of the target material is 30 mm, opposed to the target material and arranged in parallel at a distance of 50 mm.
X Thickness: Plasma is generated between a glass substrate having a thickness of 0.5 mm and the target material, and Ar ions in the plasma collide with the surface of the target material to sputter the target material. An optical recording medium protective layer having a thickness of 90 nm was formed by vapor deposition.
For the purpose of evaluating the light refractive index and the light transmittance of the optical recording medium protective layer formed as a result, the refractive index and the extinction coefficient were measured using a laser beam having a wavelength of 633 nm. The measurement results are shown in Table 1.
【００１２】ついで、上記の各種ターゲット材の耐割損
性を評価する目的で、ターゲット材へのスパッタ電力の
印加条件を、上記の１０００Ｗから２００Ｗづつ上げて
行き、この間上昇スパッタ電力毎に１分間保持する条件
とする以外は、上記の光記録媒体保護層形成条件と同一
の条件でスパッタを行い、前記ターゲット材に割れが発
生した時点の印加スパッタ電力（割れ発生臨界スパッタ
電力）を測定した。この測定結果を表１も示した。な
お、表１には上記ターゲット材の理論密度比も併せて示
した。Next, in order to evaluate the crack resistance of the various target materials, the conditions for applying the sputtering power to the target material are increased by 200 W from the above-mentioned 1000 W in increments of 200 W. Sputtering was performed under the same conditions as those for forming the optical recording medium protective layer except that the conditions were maintained, and the applied sputter power (crack generation critical sputter power) at the time when the target material cracked was measured. Table 1 also shows the measurement results. Table 1 also shows the theoretical density ratio of the target material.
【００１３】[0013]
【表１】 [Table 1]
【００１４】[0014]
【発明の効果】表１に示される結果から、本発明ターゲ
ット材１〜９は、いずれもＬａ2Ｏ3の含有によって、Ｌ
ａ2Ｏ3を含有しない従来ターゲット材１〜５に比して著
しく高い割れ発生臨界スパッタ電力値を示し、これはス
パッタ条件を高出力スパッタ条件としても割損の発生が
抑制され、保護層の高速成膜性を可能とすることを示す
ものであり、さらに本発明ターゲット材１〜９を用いて
形成された光記録媒体保護層の屈折率および消衰係数と
前記従来ターゲット材１〜５を用いて形成されたそれと
の間にほとんど変化が見られず、これはＬａ2Ｏ3の含有
によって光記録媒体保護層の特性が損なわれることがな
いことを示すものである。上述のように、この発明のタ
ーゲット材は、高出力スパッタの負荷によっても割れの
発生が抑制され、すぐれた耐割損性を示すことから、従
来光記録媒体保護層と同等の特性を具備した保護層の高
速成膜を可能とし、生産性の向上に寄与するものであ
る。According to the results shown in Table 1, all of the target materials 1 to 9 of the present invention have L 2 O 3 due to the inclusion of La 2 O 3.
It shows a significantly higher critical sputtering power value for crack generation as compared with the conventional target materials 1 to 5 which do not contain a 2 O 3 . It shows that high-speed film forming properties are possible, and furthermore, the refractive index and extinction coefficient of the optical recording medium protective layer formed using the target materials 1 to 9 of the present invention and the conventional target materials 1 to 5 There was almost no change from that formed by using this, which indicates that the content of La 2 O 3 does not impair the properties of the optical recording medium protective layer. As described above, the target material of the present invention has the same characteristics as those of the conventional optical recording medium protective layer because the generation of cracks is suppressed even by the load of high-power spatter, and it exhibits excellent breakage resistance. This enables the high-speed deposition of the protective layer and contributes to an improvement in productivity.
【図１】高周波マグネトロンスパッタリング装置を例示
する概略縦断面図である。FIG. 1 is a schematic longitudinal sectional view illustrating a high-frequency magnetron sputtering apparatus.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 森 理恵 埼玉県大宮市北袋町１−297 三菱マテリ アル株式会社総合研究所内 Ｆターム(参考） 4K029 AA11 BA41 BA43 BA46 BA64 BB02 BC08 BD12 CA05 DC05 DC09 5D029 LA14 LA15 5D121 AA04 EE09 EE11 ──────────────────────────────────────────────────の Continuing from the front page (72) Inventor Rie Mori 1-297 Kitabukuro-cho, Omiya-shi, Saitama F-term in the Mitsubishi Materials Research Laboratory (reference) 4K029 AA11 BA41 BA43 BA46 BA64 BB02 BC08 BD12 CA05 DC05 DC09 5D029 LA14 LA15 5D121 AA04 EE09 EE11
Claims (1)
体で構成したことを特徴とする、高出力スパッタ条件で
すぐれた耐割損性を発揮する光記録媒体保護層形成用ス
パッタリングターゲット焼結材。1. A hot-press sintered body of a mixed powder having a composition of mol%, silicon oxide: 6 to 40%, lanthanum oxide: 1 to 6%, zinc sulfide: remaining, Characterized by a sputtering target sintered material for forming an optical recording medium protective layer, which exhibits excellent crack resistance under high output sputtering conditions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000383022A JP2002180245A (en) | 2000-12-18 | 2000-12-18 | Sputtering target sintered material for photorecording medium protective layer exhibiting excellent cracking damage resistance in high output sputtering condition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000383022A JP2002180245A (en) | 2000-12-18 | 2000-12-18 | Sputtering target sintered material for photorecording medium protective layer exhibiting excellent cracking damage resistance in high output sputtering condition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2002180245A true JP2002180245A (en) | 2002-06-26 |
Family
ID=18850748
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000383022A Withdrawn JP2002180245A (en) | 2000-12-18 | 2000-12-18 | Sputtering target sintered material for photorecording medium protective layer exhibiting excellent cracking damage resistance in high output sputtering condition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2002180245A (en) |
-
2000
- 2000-12-18 JP JP2000383022A patent/JP2002180245A/en not_active Withdrawn
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